A fast electrochemical imaging system and method based on lower computer driving

Abstract

A kind of fast electrochemical imaging system and method based on lower machine drive belong to electrochemical measurement device field, solve the technical problems of slow imaging speed in prior art, and due to the electrochemical imaging using host computer driving strategy, leading to multithreading scheduling delay, poor synchronism and insufficient real-time nature.The fast electrochemical imaging system is built, including fast imaging controller, electrochemical workstation gear shift controller, host computer, electrochemical workstation, piezoelectric driver and experimental system, three-dimensional piezoelectric displacement table is arranged in the experimental system, by designing host computer operation software, lower machine controller and other modules, combined with experimental system, the strategy of lower machine drive imaging is realized, and a kind of electrochemical imaging method using fast electrochemical imaging system is given.The present application is used to realize fast, stable electrochemical imaging.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of electrochemical measurement devices, in particular to a rapid electrochemical imaging system and method based on lower machine driving. BACKGROUND

[0002] SECM (Scanning Electrochemical Microscopy) technology is based on classical electrochemistry (electrode reaction kinetics and material diffusion), and reflects the concentration gradient of redox substances near the probe tip through the Faraday current of the probe, which is used to detect the (electro) chemical reaction activity and chemical microenvironment of the sample surface. The biggest difference between electrochemical imaging technology represented by SECM and STM (Scanning Tunneling Microscope) and AFM (Atomic Force Microscope) and other technologies is that SECM detects electrochemical activity (chemical function), while STM and AFM detect physical and chemical structure and properties.

[0003] For scanning probe imaging technology, whether it is topography imaging based on STM and AFM, or electrochemical imaging based on SECM, slow scanning speed is a very critical problem in practical application. Lower time resolution makes it difficult to observe fast dynamic processes, and low scanning speed limits the size of the imaging range and also puts high requirements on the stability of the imaging sample. Especially for electrochemical imaging based on SECM, slow scanning will interfere with the local concentration field of the substrate surface, exacerbate the pollution and passivation of the substrate or probe caused by the by-products of the electrochemical reaction, and make the subsequent scanning meaningless. Moreover, high-resolution SECM imaging usually needs to combine Approach Curve (Approach Curve) to accurately determine the probe-substrate distance or obtain local kinetic information. It takes time (usually several seconds to tens of seconds) to obtain a high-quality approach curve at each imaging point or key area. If high-density, multi-point approach measurement is performed on the entire image, the time required under slow scanning will become extremely long (possibly several hours), making this method almost infeasible in practical applications, especially when studying unstable systems.

[0004] Currently, some studies have adopted the strategy of lower machine control to improve the imaging scanning speed of AFM and STM. However, the current SECM-based electrochemical imaging still mainly adopts the host computer driving strategy. The research methods for improving the imaging rate focus on optimizing the hardware design, imaging path and imaging algorithm, and developing advanced electrodes (multi-channel array), such as the prior art, Chinese patent document CN113670997A discloses a "scanning electrochemical microscope path planning method and device based on script analysis" to optimize the imaging path, and Chinese patent document CN114518070A discloses a "fast positioning method and system of a scanning probe microscope system" to plan the imaging algorithm, but the improvement methods of imaging path optimization and imaging algorithm optimization are accompanied by the loss of sample surface information and spatial resolution, and the improvement level of imaging rate is limited.

[0005] Therefore, although these methods can improve the imaging rate to different extents, there are still limitations, mainly manifested as the existence of multi-thread scheduling delay, poor real-time performance and other problems in the underlying running logic of the host computer driving, which makes it difficult to realize the efficient cooperation of the signal acquisition, motion control and electrochemical measurement function modules, and fundamentally improves the imaging rate.

[0006] In summary, the prior art has the technical problems of slow imaging speed and poor real-time performance due to the use of host computer driving strategy for electrochemical imaging. SUMMARY

[0007] The present application solves the technical problems of slow imaging speed and poor real-time performance due to the use of host computer driving strategy for electrochemical imaging.

[0008] The fast electrochemical imaging system based on lower machine driving according to the present application comprises a fast imaging controller, a gear shifting controller, a host computer, an electrochemical workstation, an experimental system and a piezoelectric driver, wherein the experimental system is provided with a three-dimensional piezoelectric displacement stage.

[0009] The host computer transmits experimental parameters to the fast imaging controller and transmits gear shifting parameters to the gear shifting controller.

[0010] The fast imaging controller receives experimental parameters, processes them to generate voltage signals and position control signals, transmits the voltage signals to the electrochemical workstation, transmits the position control signals to the piezoelectric driver, collects real-time position data and real-time current of the electrochemical imaging experiment, and transmits the processed data to the host computer.

[0011] The piezoelectric driver receives a position control signal for controlling displacement of the three-dimensional piezoelectric displacement stage, and receives real-time position data returned by the three-dimensional piezoelectric displacement stage and transmits the real-time position data to the rapid imaging controller;

[0012] The three-dimensional piezoelectric displacement stage moves based on the position control signal to obtain the real-time position data and returns the real-time position data to the piezoelectric driver;

[0013] The gear switching controller receives the gear switching parameter, processes the gear switching parameter, and transmits the processed gear switching parameter to the electrochemical workstation;

[0014] The electrochemical workstation receives the processed gear switching parameter, controls gear switching and channel start-stop, receives a voltage signal, applies the voltage signal to an electrochemical imaging experiment, collects real-time current of the electrochemical imaging experiment, and transmits the real-time current to the rapid imaging controller.

[0015] Further, in an embodiment of the present application, the host computer includes an electrochemical experiment parameter setting unit, an electrochemical workstation gear switching module unit, an experiment data storage unit, and an experiment data observation unit;

[0016] The electrochemical experiment parameter setting unit sets experiment parameters and transmits the experiment parameters to the rapid imaging controller;

[0017] The electrochemical workstation gear switching module unit sets gear switching parameters and transmits the gear switching parameters to the gear switching controller;

[0018] The experiment data storage unit sets a storage path and a file name of processed collected data transmitted by the rapid imaging controller;

[0019] The experiment data observation unit observes and displays processed collected data transmitted by the rapid imaging controller.

[0020] Further, in an embodiment of the present application, the rapid imaging controller includes a position control module, an information collection module, and an electrochemical signal control module;

[0021] The position control module transmits a position control signal to the piezoelectric driver;

[0022] The electrochemical signal control module transmits a voltage signal to the electrochemical workstation;

[0023] The information collection module collects real-time position data and real-time current of an electrochemical imaging experiment.

[0024] Further, in an embodiment of the present application, the rapid imaging controller further includes a first power supply circuit module, a first core single-chip microcomputer module, a first serial port module, and a first circuit function module.

[0025] The first power supply circuit module is used for power supply of the fast imaging controller;

[0026] The first core single-chip microcomputer module is used for performing the function task of the fast imaging controller lower computer;

[0027] The first serial port module is used for communication between the fast imaging controller lower computer and the upper computer;

[0028] The first circuit function module is used for program burning, hardware reset and anti-static protection of the fast imaging controller.

[0029] Further, in an embodiment of the present application, the gear shifting controller comprises a second power supply circuit module, a second core single-chip microcomputer module, a second serial port module, an 8-way voltage output module and a second circuit function module;

[0030] The second power supply circuit module is used for power supply of the gear shifting controller;

[0031] The second core single-chip microcomputer module is used for performing the function task of the gear shifting controller lower computer;

[0032] The second serial port module is used for communication between the gear shifting controller lower computer and the upper computer;

[0033] The 8-way voltage output module is used for transmitting the processed gear shifting parameters to the electrochemical workstation;

[0034] The second circuit function module is used for program burning, hardware reset and anti-static protection of the gear shifting controller.

[0035] The present application discloses a fast electrochemical imaging method based on lower computer driving.

[0036] Step 1, setting experiment parameters and gear shifting parameters of the upper computer interface program;

[0037] Step 2, receiving and processing the experiment parameters by the fast imaging controller to obtain processed experiment parameters;

[0038] Step 3, receiving and transmitting the gear shifting parameters by the gear shifting controller to control gear shifting and channel start-stop of the electrochemical imaging experiment;

[0039] Step 4, performing the electrochemical imaging experiment based on the processed experiment parameters and the gear shifting parameters to obtain real-time position data and real-time current;

[0040] Step 5, receiving and processing real-time position data and real-time current by using the fast imaging controller, transmitting to the host computer after processing for real-time display and storage.

[0041] Further, in one embodiment of the present application, the experimental parameters include channel 1 initial voltage, channel 2 initial voltage, infinite asymptotic step, feedback zone asymptotic step, negative feedback stop current level, channel 1 sensitivity, channel 2 sensitivity, XY imaging area, X-axis step and Y-axis step.

[0042] Further, in one embodiment of the present application, the step 4 of performing electrochemical imaging experiment based on the processed experimental parameters and gear switching parameters includes the following steps:

[0043] Step 41, obtaining position control signal and voltage signal by using the fast imaging controller to process the experimental parameters;

[0044] Step 42, transmitting the position control signal to the piezoelectric driver based on the position control module, and the piezoelectric driver controls the displacement of the three-dimensional piezoelectric displacement stage by using the position control signal;

[0045] Step 43, transmitting the voltage signal to the electrochemical workstation based on the electrochemical signal control module, and applying the voltage signal to the electrochemical imaging experiment;

[0046] Step 44, performing electrochemical imaging experiment based on the displacement of the three-dimensional piezoelectric displacement stage and the application of the voltage signal.

[0047] The present application solves the technical problems of slow imaging speed in the prior art, and due to the use of host computer driving strategy for electrochemical imaging, resulting in large multi-thread scheduling delay, poor synchronization and insufficient real-time performance. The specific beneficial effects include:

[0048] 1、The present application proposes a fast electrochemical imaging system based on lower computer driving, and the prior art uses host computer driving strategy for electrochemical imaging, resulting in large multi-thread scheduling delay, poor synchronization and insufficient real-time performance, in order to solve the above problems, the present application designs fast imaging controller and electrochemical workstation gear switching controller and other lower computer end, divides the imaging function into modules, realizes the mutual independence and efficient work of upper and lower computer functions, the host computer in the system only undertakes the task of experimental parameter delivery and data display and storage, and the lower computer is responsible for the task execution of imaging experiment, which can realize simple and efficient imaging process, and the signal acquisition rate of this lower computer driving strategy can reach 200 K, and the imaging response time can reach millisecond level during experiment, which is more than 5 times higher than that of the host computer driving strategy.

[0049] 2. The application provides a fast electrochemical imaging method based on lower machine driving, which realizes optimization of an imaging path through innovative ideas of refining imaging parameter setting and dynamically adjusting imaging progressive step length.

[0050] The fast electrochemical imaging system and the fast electrochemical imaging method are combined, and under the joint action of the improvement of imaging response time and the optimization of the imaging path, the imaging rate can be improved under different experimental scenes and experimental schemes, has universality, and can further improve the imaging speed, and realizes 20-100 times improvement. BRIEF DESCRIPTION OF DRAWINGS

[0051] The above and / or additional aspects and advantages of the present application will become apparent and more readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings, in which:

[0052] Figure 1 is a schematic diagram of the fast electrochemical imaging system of embodiment one;

[0053] Figure 2 is a design schematic diagram of the upper computer program constant height imaging interface electrochemical experiment parameter setting unit 100 and the electrochemical workstation gear switching module unit 200 of embodiment two;

[0054] Figure 3 is a design schematic diagram of the upper computer program constant height imaging interface experiment data storage unit 300 of embodiment two;

[0055] Figure 4 is a design schematic diagram of the upper computer program constant height imaging interface experiment data observation unit 400 of embodiment two;

[0056] Figure 5 is a design schematic diagram of the upper computer program PAC progressive interface electrochemical experiment parameter setting unit 100 and the electrochemical workstation gear switching module unit 200 of embodiment two;

[0057] Figure 6 is a design schematic diagram of the upper computer program PAC progressive interface experiment data storage unit 300 of embodiment two;

[0058] Figure 7 is a design schematic diagram of the upper computer program PAC progressive interface experiment data observation unit 400 of embodiment two;

[0059] Figure 8 is a fast imaging controller unit of embodiment three;

[0060] Figure 9 is an electrochemical workstation gear switching controller unit of embodiment four;

[0061] Figure 10 is a running logic framework diagram of the fast electrochemical imaging system according to embodiment five;

[0062] Figure 11 is a running logic framework diagram of the fast imaging controller according to embodiment three;

[0063] Figure 12 is a running logic framework diagram of the electrochemical workstation gear switching controller according to embodiment four;

[0064] Figure 13 is the collected X-Y-i current distribution data according to embodiment seven;

[0065] Figure 14 is the converted X-Y-Z topography distribution data according to embodiment seven. DETAILED DESCRIPTION

[0066] Various embodiments of the present application will be described in detail below with reference to the accompanying drawings. The examples described by reference to the accompanying drawings are exemplary and are intended to explain the present application, and should not be understood as limiting the present application.

[0067] Embodiment one

[0068] A fast electrochemical imaging system based on lower computer driving, comprising a fast imaging controller 500, a gear switching controller 600, an upper computer 700, an electrochemical workstation 800, an experimental system 900, and a piezoelectric driver 1000, wherein the experimental system 900 is provided with a three-dimensional piezoelectric displacement stage 901;

[0069] The upper computer 700 transmits experimental parameters to the fast imaging controller 500 and transmits gear switching parameters to the gear switching controller 600;

[0070] The fast imaging controller 500 receives experimental parameters, processes them to generate voltage signals and position control signals, transmits the voltage signals to the electrochemical workstation 800, transmits the position control signals to the piezoelectric driver 1000, collects real-time position data and real-time current of the electrochemical imaging experiment, and transmits the collected data to the upper computer 700 after processing;

[0071] The piezoelectric driver 1000 receives position control signals for controlling the displacement of the three-dimensional piezoelectric displacement stage 901, and receives real-time position data returned by the three-dimensional piezoelectric displacement stage 901 and transmits them to the fast imaging controller 500;

[0072] The three-dimensional piezoelectric displacement stage 901 moves based on the position control signals and returns real-time position data to the piezoelectric driver 1000;

[0073] The gear shift controller 600 receives the gear shift parameters, processes and transmits them to the electrochemical workstation 800.

[0074] The electrochemical workstation 800 receives the processed gear shift parameters, controls the gear shift and channel start-stop, receives the voltage signal, applies the voltage signal for electrochemical imaging experiments, collects real-time current for electrochemical imaging experiments, and transmits them to the fast imaging controller 500.

[0075] Although existing imaging technology has used the strategy of driving the lower computer such as STM32 to improve the imaging rate, this strategy is mostly for AFM and STM imaging technology, and lacks research on SECM-based electrochemical imaging technology. Existing research on improving electrochemical imaging speed mostly focuses on hardware design optimization, advanced electrode (multi-channel array) development, imaging path optimization, and imaging algorithm optimization. These researches have limited effect on improving imaging speed and are not universal. Hardware design optimization and advanced electrode development have strict requirements on process, instrument complexity, and cost, and are limited in spatial resolution. Imaging path optimization and imaging algorithm optimization have limited effect on improving imaging speed, and traditional electrochemical imaging systems mostly use upper computer driving architecture, which has problems such as long response delay, poor synchronization, and insufficient real-time performance, which severely limits the level of dynamic information that can be recorded and obtained during imaging.

[0076] To solve the above problems, the present embodiment proposes a fast electrochemical imaging system based on lower computer driving, as shown in Figure 1 The fast imaging controller 500, gear shift controller 600, and other lower computer ends are designed by embedded development method, the imaging function is divided into modules, the upper and lower computer functions are independent and work efficiently, the fast electrochemical imaging strategy driven by lower computer greatly reduces the long response time of the original upper computer control strategy, and the electrochemical imaging speed is greatly improved. The construction of the fast electrochemical imaging system includes the following steps:

[0077] Step 1: Fix the fast imaging controller 500, gear shift controller 600, and piezoelectric driver 1000 in the square panel box.

[0078] Step 2: Connect the fast imaging controller 500, gear shift controller 600, and upper computer 700 (experimental computer) through two data lines.

[0079] Step 3, connect the position control module 505 interface of the fast imaging controller 500 with the piezoelectric driver 1000 input interface, and then connect the piezoelectric driver 1000 with the three-dimensional piezoelectric displacement platform 901 in the MT-SRECM100 experimental system 900. Transmit the position control signal to the piezoelectric driver 1000 through the fast imaging controller 500, and then output the position control signal to the three-dimensional piezoelectric displacement platform 901 through the piezoelectric driver 1000, so as to realize the position response and control of XYZ during the imaging process.

[0080] Step 4, connect the information acquisition module 506 interface of the fast imaging controller 500 with the piezoelectric driver 1000 output interface, and acquire the real-time position data of XYZ from the three-dimensional piezoelectric displacement platform 901 during the position control process.

[0081] Step 5, connect the electrochemical signal control module 504 interface of the fast imaging controller 500 with the electrochemical workstation 800 input interface. After the connection is completed, the related electrochemical signal (such as the voltage applied to the electrode) can be applied to the imaging experimental target end through the electrochemical workstation 800.

[0082] Step 6, use the signal line to connect the 8-way voltage output module 604 of the gear shifting controller 600 with the electrochemical workstation 800. The gear shifting controller 600 outputs different high-low level combination signals to the electrochemical workstation 800 through the 8-way output, so as to realize the switching and starting and stopping of the channels of the electrochemical workstation 800 during the imaging experiment.

[0083] Step 7, download the prepared fast imaging controller program and gear shifting controller program to the respective main control units, so as to drive the subsequent electrochemical imaging experiment.

[0084] Step 8, connect the assembled panel box to the MT-SRECM100 experimental system 900, turn on the power, start the modules, and complete the construction of the fast electrochemical imaging system.

[0085] Therefore, the embodiment provides a fast electrochemical imaging system based on the driving of the lower computer. Through the construction and design of the fast electrochemical imaging system, the fast electrochemical imaging system includes the specific connection scheme and operation steps of the fast imaging controller 500, the gear shifting controller 600, the upper computer 700, the electrochemical workstation 800, the experimental system 900 and the piezoelectric driver 1000, and solves the technical problems of large multi-thread scheduling delay, poor synchronization and insufficient real-time performance caused by the electrochemical imaging driven by the upper computer in the prior art.

[0086] Embodiment two

[0087] The embodiment is a further limitation of the fast electrochemical imaging system based on the lower machine drive of the embodiment one, and the host computer 700 includes an electrochemical experiment parameter setting unit 100, an electrochemical workstation gear shifting module unit 200, an experiment data storage unit 300 and an experiment data observation unit 400.

[0088] In the traditional method, the host computer program also needs to drive the imaging function, which limits the rapid acquisition of data and the rapid execution of commands. In order to solve the above problems, the host computer interface program in the embodiment only undertakes the functions of experiment parameter setting and transmission, that is, data transmission, as shown in Figure 2 、 Figure 3 and Figure 4 , it is a schematic diagram of the constant height imaging interface design of the host computer program, as shown in Figure 5 、 Figure 6 and Figure 7 , it is a schematic diagram of the PAC progressive interface design of the host computer program. The host computer interface program developed based on LabVIEW (laboratory virtual instrument engineering workbench) in the embodiment includes each specific experiment parameter interface and design of electrochemical imaging, and each specific gear shifting parameter interface and design of gear shifting.

[0089] The electrochemical experiment parameter setting unit 100 is used for setting experiment parameters and transmitting to the fast imaging controller 500. The parameters include: imaging mode (positive feedback, negative feedback), stop current level corresponding to the imaging mode, standing time before imaging starts and reference current collection time, initial voltage of channel 1 and initial voltage of channel 2 applied to the probe at the imaging start, channel 1 sensitivity and channel 2 sensitivity corresponding to the current collected in the experiment, sampling interval in the imaging process, initial position of the probe Z axis in the imaging process, progressive step length at the infinite distance of the Z axis and progressive step length in the feedback area of the Z axis, actual scanning imaging direction and XYZ standing time after the progress is completed, X axis start point, X axis end point and X axis step length of the imaging area, Y axis start point, X axis end point and X axis step length of the imaging area, X axis start point, X axis end point, Y axis start point and Y axis end point of the imaging area, which constitute an XY imaging area.

[0090] The electrochemical workstation gear shifting module unit 200 is used for setting gear shifting parameters and transmitting to the gear shifting controller 600. The parameters include: channel 1 sensitivity and channel 2 sensitivity corresponding to the current collected in the experiment, wherein the sensitivity options are 10 R, 100 R, 1 K, 10 K, 100 K, 1 M, 10M, 100 M, 1 G, 10 G, 100 G and 1 T, which correspond to different current ranges, and a gear shifting serial port setting module.

[0091] The experimental data storage unit 300 is configured to set a storage path of the data transmitted by the fast imaging controller 500, and includes selecting a storage path of the imaging data of the experimental data, naming the imaging data file, and naming the PAC (probe) progressive process data file.

[0092] The experimental data observation unit 400 is configured to observe and display the data transmitted by the fast imaging controller 500, and mainly includes PAC static time observation, X / Y static time observation, Z-axis static time observation during imaging, X current position detection, Y current position detection, and Z current position detection, reference current detection, positive feedback current stop level detection, negative feedback current stop level detection, last stop current of channel 1, current of channel 1, last stop current of channel 2, current of channel 2, Z-axis step length, total imaging point number detection, and current imaging point number detection, X-Y-i real-time data display module, X-Y-Z real-time data display module, and PAC real-time data display module.

[0093] Embodiment three

[0094] The embodiment is a further limitation of the fast electrochemical imaging system based on the lower machine drive according to the embodiment one, and the fast imaging controller 500 includes a position control module 505, an information acquisition module 506, an electrochemical signal control module 504, a first power supply circuit module 501, a first core single-chip microcomputer module 502, a first serial port module 503, and a first circuit function module 507.

[0095] The position control module 505 based on the DAC (Digital-to-Analog Converter)-based digital-to-analog conversion circuit transmits a position control signal to the piezoelectric driver 1000, and is configured to control the displacement of the three-dimensional piezoelectric displacement stage 901.

[0096] The electrochemical signal control module 504 based on the DAC-based digital-to-analog conversion circuit is configured to transmit relevant electrochemical signal parameters in the imaging experiment, and transmit a voltage signal to the electrochemical workstation 800.

[0097] The information acquisition module 506 based on the ADC (Analog-to-Digital Converter)-based analog-to-digital conversion circuit is configured to acquire real-time position data in the piezoelectric driver 1000 and electrochemical parameters of the electrochemical imaging experiment.

[0098] The first power supply circuit module 501 is configured to supply power to the control unit of the fast imaging controller 500, various chips, sensors, and the like.

[0099] The first core single-chip microcomputer module 502 (STM32) is used for performing the function task of the lower computer of the fast imaging controller 500.

[0100] The first serial port module 503 (USB-to-serial port circuit and full-speed USB experimental test circuit) is used for the communication between the lower computer of the fast imaging controller 500 and the upper computer.

[0101] The first circuit function module 507 is used for the program burning, hardware reset and anti-static protection of the fast imaging controller 500.

[0102] The fast imaging controller 500 based on embedded development in the embodiment includes the selection of the single-chip microcomputer, various sensor chips, the circuit design of each module and the PCB (printed circuit board) design of the fast imaging controller, and the operation control logic of the upper computer interface program and the fast imaging controller 500, as shown in FIGS. 1 to 3. Figure 8 and Figure 11 As shown in FIGS. 1 to 3, the fast imaging controller 500 is used for receiving the experimental parameters transmitted by the upper computer 700, processing the experimental parameters, generating a voltage signal and transmitting the voltage signal to the electrochemical workstation 800, generating a position control signal to the piezoelectric driver 1000, collecting real-time position data in the piezoelectric driver 1000 and real-time current of the electrochemical imaging experiment, processing the real-time position data and the real-time current, and transmitting the processed real-time position data and the real-time current to the upper computer 700 for real-time display and storage.

[0103] Embodiment Four

[0104] The embodiment is a further limitation of the fast electrochemical imaging system based on lower computer driving in the embodiment one, and the gear shifting controller 600 includes a second power supply circuit module 601, a second core single-chip microcomputer module 602, a second serial port module 603, an 8-way voltage output module 604 and a second circuit function module 605.

[0105] The second power supply circuit module 601 is used for supplying power to the control unit of the gear shifting controller 600, various chips and sensors and the like.

[0106] The second core single-chip microcomputer module 602 (STM32) is used for performing the function task of the lower computer of the gear shifting controller 600.

[0107] The second serial port module 603 (USB-to-serial port circuit) is used for the communication between the lower computer of the gear shifting controller 600 and the upper computer.

[0108] The 8-way voltage output module 604 is used for transmitting the processed gear shifting parameters to the electrochemical workstation 800 to control the gear shifting and the channel opening.

[0109] The second circuit function module 605 is used for program burning, hardware reset and anti-static protection of the gear shifting controller 600.

[0110] The gear shifting controller 600 based on embedded development in the embodiment includes a single-chip microcomputer, selection of various sensor chips, circuit design of each function module, PCB design of the gear shifting controller 600, and operation control logic of the upper computer interface program and the electrochemical workstation gear shifter 600, as shown in Figure 9 and Figure 12 As shown in the figure, the gear shifting controller 600 receives the gear shifting parameters transmitted by the upper computer 700, processes the gear shifting parameters, and transmits the processed gear shifting parameters to the electrochemical workstation 800 for controlling gear shifting and channel start-stop.

[0111] Embodiment five

[0112] The rapid electrochemical imaging method based on lower computer driving in the embodiment is implemented based on the system in the embodiments one to four, and includes the following steps.

[0113] Step 1, setting experiment parameters and gear shifting parameters of the upper computer 700 interface program;

[0114] Step 2, receiving experiment parameters by the rapid imaging controller 500 and processing the experiment parameters to obtain processed experiment parameters;

[0115] Step 3, receiving and transmitting gear shifting parameters by the gear shifting controller 600 to control gear shifting and channel start-stop of the electrochemical imaging experiment;

[0116] Step 4, performing electrochemical imaging experiment based on the processed experiment parameters and gear shifting parameters to obtain real-time position data and real-time current;

[0117] Step 5, receiving and processing real-time position data and real-time current by the rapid imaging controller 500, and transmitting the processed data to the upper computer 700 for real-time display and storage.

[0118] The step 4 of performing electrochemical imaging experiment based on the processed experiment parameters and gear shifting parameters includes the following steps.

[0119] Step 41, obtaining position control signals and voltage signals by processing experiment parameters by the rapid imaging controller 500;

[0120] Step 42, transmitting the position control signals to the piezoelectric driver 1000 based on the position control module 505, and controlling displacement of the three-dimensional piezoelectric displacement stage 901 by the piezoelectric driver 1000 using the position control signals;

[0121] Step 43, the electrochemical signal control module 504 transmits a voltage signal to the electrochemical workstation 800 based on the electrochemical signal control module 504, and the voltage signal is applied to the electrochemical imaging experiment;

[0122] Step 44, based on the displacement of the three-dimensional piezoelectric displacement stage 901 and the application of the voltage signal, the electrochemical imaging experiment is carried out.

[0123] As Figure 10 shown, based on the rapid electrochemical imaging system, the operation logic of the rapid electrochemical imaging method described in the embodiment is as follows:

[0124] The experimenter inputs the imaging experiment parameters on the host computer interface program, selects the electrochemical gear and channel information, data saving file and path information, and clicks to send. The data is sent to the serial port through the USB, and the lower computer end (rapid imaging controller 500 and gear switching controller 600) receives and processes it.

[0125] The rapid imaging controller 500 receives and processes the imaging experiment parameters, sends a position control signal to the piezoelectric driver 1000, and then drives the three-dimensional piezoelectric displacement stage 901 to move, thereby realizing the position movement of the working probe during the imaging experiment. At the same time, the voltage signal is sent to the electrochemical workstation 800, so that it outputs the set experimental voltage signal value, realizing the application of the electrochemical signal in the imaging experiment.

[0126] The gear switching controller 600 receives and processes the gear switching parameters, outputs the corresponding combination of 8-way output level signals, and transmits them to the electrochemical workstation 800 through the signal line. The electrochemical workstation 800 receives the signal, realizes the switching of the gear and the start and stop of the channel.

[0127] After the experiment starts, the XYZ real-time position data (voltage signal) of the three-dimensional piezoelectric displacement stage 901 is returned to the piezoelectric driver 1000 in real time, the piezoelectric driver 1000 outputs the real-time position data to the rapid imaging controller 500, and is collected by it. The rapid imaging controller 500 processes the data, outputs the current position information and sends it to the host computer end through the data line, and displays and stores it in real time.

[0128] The electrochemical workstation 800 detects the real-time current during the experiment and processes it to obtain the current current information, which is transmitted to the rapid imaging controller 500 for processing and then sent to the host computer interface program through the data line, and displayed and stored in real time.

[0129] To sum up, the application adopts the new method of lower machine driving, and through improving the speed of electrochemical imaging experiment, can help to solve the experimental difficulties such as sample aging, probe and sample pollution, drift, and help to realize higher space-time resolution electrochemical imaging. And the fast electrochemical imaging system and the fast electrochemical imaging method have universality, and can realize the improvement of imaging rate under different experimental scenes and experimental schemes.

[0130] Embodiment six

[0131] The PAC test is carried out based on the fast electrochemical imaging system and the fast electrochemical imaging method in embodiments one to five, and the purpose of the embodiment is to test the imaging speed of the designed fast electrochemical imaging system based on lower machine driving, and compare it with the imaging speed of the traditional upper machine driving electrochemical imaging method, and then verify the feasibility of the application, which specifically includes the following steps:

[0132] Step 1, open the upper machine interface program, set the imaging data storage path, customize the imaging file name and PAC file name, and open the file saving button;

[0133] Step 2, set the PAC gradual program related parameters in the traditional mode, wherein the Z-axis initial position is set to 0, the Z-axis gradual step is set to 0.1 μm, and the Z-axis gradual process is 40 μm, the Z-axis gradual step includes the Z-axis infinite gradual step and the Z-axis feedback zone gradual step, both of which are set to 0.1 μm;

[0134] Step 3, take the prepared 500 nm carbon nanometer electrode, fix it on the three-dimensional piezoelectric displacement table 901, and connect the working electrode 1 of the electrochemical workstation 800, the reference electrode and the counter electrode of the electrochemical workstation 800 are connected with the Ag / AgCl wire, and the working electrode two is not connected. The purpose of this step is to ensure that the test is carried out in a real experimental scene;

[0135] Step 4, after completing the experimental scene construction, click the start button in the program to start the PAC imaging experiment;

[0136] Step 5, using the fast electrochemical imaging system, repeating the steps 1 to 4 of the embodiment, comparing and testing in the same experimental scene, that is, keeping the experimental parameters the same, using the same electrode and controlling the experimental variables consistent;

[0137] Step 6, comparing the experimental results under the two methods, the response time between each step of the three-dimensional moving platform in the traditional mode is about 0.2 s, and the response time between each step of the three-dimensional piezoelectric displacement table 901 in the mode of the embodiment is about 40-50 ms.

[0138] The experimental results show that the rapid electrochemical imaging system can greatly shorten the response time between each step of the three-dimensional moving platform, and the imaging efficiency is improved by five times.

[0139] Embodiment seven

[0140] Based on the rapid electrochemical imaging system and the rapid electrochemical imaging method described in embodiments one to five, a new imaging path optimization method is proposed, which optimizes the total speed of the probe in the imaging process by customizing the speed of the progressive process (fast stepping at infinity, slow stepping in the feedback zone), and realizes the improvement of the imaging speed. This rapid imaging method based on the lower computer drive and the path optimization under the specific imaging mode specifically includes the following steps:

[0141] Step 1, start the MT-SRECM100 experimental system 900 and build the experimental environment.

[0142] Place the non-conductive standard grating sample on the stage, and fix the working probe (2 μm carbon micrometer electrode) on the three-dimensional piezoelectric displacement table 901.

[0143] Step 2, electrochemical workstation 800, wherein the working electrode 1 is connected to the working probe, the reference electrode and the counter electrode are connected to the Ag / AgCl (silver / chloride) wire, and a two-electrode experimental system is formed.

[0144] Step 3, through the optical side microscope of the MT-SRECM100 experimental system 900, the position information of the working probe and the grating sample is obtained, and they are adjusted to the appropriate position (more than 10 times the size of the working probe) and the stage is fixed.

[0145] Step 4, immerse the two-electrode experimental system in an electrolyte solution containing 1 mmol L -1 FcMeOH (ferrocene methanol) and 0.1 mol L -1 KCl (potassium chloride), complete the experimental environment building.

[0146] Step 5, open the upper computer interface program and select the jump imaging mode.

[0147] Step 6, configure the experimental parameters, and the related core parameter settings are as follows: channel one initial voltage 0.4 V, infinite progressive step length 0.1 μm, feedback zone progressive step length 0.05 μm, realize the optimization of the imaging path; negative feedback stop current level 0.2; channel 1 sensitivity 1 G (0-5 nA); XY imaging area 40*40 μm; X axis step length and Y axis step length are both 2 μm.

[0148] Step 7, close the MT-SRCM 100 experimental system 900 Faraday box, click the host computer software start button, the host computer 700 sends the experimental parameters to the fast imaging controller 500 and the gear switching controller 600, drives the start of the experiment after processing, and performs the SECM negative feedback jump experiment.

[0149] Step 8, observe the experimental real-time data of the host computer interface program, judge whether the experiment is successful through real-time current size and real-time position information, and wait for the experiment to be completed.

[0150] Step 9, obtain experimental data, process the experimental data, and obtain the SECM negative feedback jump imaging result of the standard grating.

[0151] The response speed between each step of the PAC test in the sixth embodiment is increased to 5 times. On this basis, the jump imaging mode of the present embodiment can further shorten the imaging point number and imaging time by optimizing the imaging path, i.e. setting different progressive step lengths, and controlling the jump progressive number. Figure 13 As shown in the figure, the X-Y-i current distribution data collected is shown, wherein I (nA) is the current (nanoampere), P (um)-x and P (um)-y are the x-axis direction and the y-axis direction respectively, and Figure 14 As shown in the figure, the X-Y-Z topography distribution data obtained by conversion calculation is shown, wherein P (um)-x and P (um)-y are the x-axis direction and the y-axis direction respectively, and L (D / a) is the z-axis direction, representing the distance D between the working probe and the base compared with the probe radius a. After calculation, the imaging speed of the present embodiment can be increased by more than 20-100 times compared with the traditional method in the jump imaging mode. The more the jump number in the jump imaging, the more obvious the imaging speed improvement of the present embodiment.

[0152] Compared with the prior art, the present application has the following advantages:

[0153] 1. The present application is based on the embedded technology to design and develop a fast electrochemical imaging system and method based on the lower computer driving. Compared with the traditional host computer driving imaging strategy, the present application has high real-time performance, low delay and high synchronization accuracy, and shows significant advantages in signal acquisition, control execution and system integration, and can realize the fast response and acquisition of signals in the imaging process;

[0154] 2. Based on the advantages of the lower computer driving, the imaging rate is greatly improved, and the imaging space-time resolution is higher;

[0155] 3. The present application has high design integration and strong function coupling. The host computer only undertakes the tasks of experimental parameter delivery and data display and storage, and the lower computer is responsible for the task execution of the imaging experiment, so that the imaging process is simple and efficient.

[0156] 4、The application has strong interaction, realizes man-machine interaction through the host computer interface, and is very simple and clear in changing experimental parameters, real-time display and data storage, etc.

[0157] 5、The application has strong compatibility, and is not aimed at some specific chemical experiment scene, has strong universality, and can be used for scanning SECCM (electrochemical liquid cell microscope), scanning SICM (ion conductance microscope), SICM-SECM and SECM-SECCM and other electrochemical imaging techniques.

[0158] The above describes in detail the fast electrochemical imaging system and method based on the slave machine driving proposed in the application, the principle and implementation mode of the application are described by using specific examples, and the above embodiment description is only used to help understand the method and core idea of the application; meanwhile, for those skilled in the art, the specific implementation mode and application range will be changed according to the idea of the application, and the above description should not be understood as limiting the application.

Claims

1. A fast electrochemical imaging system based on slave machine driving, characterized in that, The application relates to a rapid imaging control device (500), a gear switching control device (600), a host computer (700), an electrochemical workstation (800), an experimental system (900) and a piezoelectric driver (1000), wherein the experimental system (900) is provided with a three-dimensional piezoelectric displacement table (901); The host computer (700) transmits experimental parameters to the rapid imaging control device (500) and transmits gear switching parameters to the gear switching control device (600); The rapid imaging control device (500) receives experimental parameters, generates voltage signals and position control signals after processing, transmits the voltage signals to the electrochemical workstation (800), transmits the position control signals to the piezoelectric driver (1000), collects real-time position data and real-time currents of electrochemical imaging experiments, and transmits the collected data to the host computer (700) after processing; The piezoelectric driver (1000) receives position control signals, controls the displacement of the three-dimensional piezoelectric displacement table (901), receives real-time position data returned by the three-dimensional piezoelectric displacement table (901) and transmits the real-time position data to the rapid imaging control device (500); The three-dimensional piezoelectric displacement table (901) moves based on the position control signals and returns real-time position data to the piezoelectric driver (1000); The gear switching control device (600) receives gear switching parameters, transmits the gear switching parameters to the electrochemical workstation (800) after processing; The electrochemical workstation (800) receives the processed gear switching parameters, controls gear switching and channel start-stop, receives voltage signals, applies the voltage signals to electrochemical imaging experiments, collects real-time currents of the electrochemical imaging experiments and transmits the real-time currents to the rapid imaging control device (500).

2. The fast electrochemical imaging system based on lower computer driving according to claim 1, wherein, The host computer (700) comprises an electrochemical experiment parameter setting unit (100), an electrochemical workstation gear switching module unit (200), an experimental data storage unit (300) and an experimental data observation unit (400); The electrochemical experiment parameter setting unit (100) is used for setting experimental parameters and transmitting the experimental parameters to the rapid imaging control device (500); The electrochemical workstation gear switching module unit (200) is used for setting gear switching parameters and transmitting the gear switching parameters to the gear switching control device (600); The experimental data storage unit (300) is used for setting a storage path and a file name of collected data transmitted by the rapid imaging control device (500) after processing; The experimental data observation unit (400) is used for observing and displaying the collected data transmitted by the rapid imaging control device (500) after processing.

3. The fast electrochemical imaging system based on lower computer driving according to claim 1, wherein, The rapid imaging control device (500) comprises a position control module (505), an information collection module (506) and an electrochemical signal control module (504); The position control module (505) transmits position control signals to the piezoelectric driver (1000); The electrochemical signal control module (504) transmits voltage signals to the electrochemical workstation (800); The information collection module (506) is used for collecting real-time position data and real-time currents of electrochemical imaging experiments.

4. The fast electrochemical imaging system based on lower computer driving according to claim 3, wherein, The rapid imaging controller (500) further comprises a first power supply circuit module (501), a first core single-chip microcomputer module (502), a first serial port module (503) and a first circuit function module (507); The first power supply circuit module (501) is used for power supply of the rapid imaging controller (500); The first core single-chip microcomputer module (502) is used for performing a function task of a lower computer of the rapid imaging controller (500); The first serial port module (503) is used for communication between the lower computer of the rapid imaging controller (500) and an upper computer; The first circuit function module (507) is used for program burning, hardware reset and anti-static protection of the rapid imaging controller (500).

5. The fast electrochemical imaging system based on lower computer driving according to claim 1, wherein, The gear switching controller (600) comprises a second power supply circuit module (601), a second core single-chip microcomputer module (602), a second serial port module (603), an 8-way voltage output module (604) and a second circuit function module (605); The second power supply circuit module (601) is used for power supply of the gear switching controller (600); The second core single-chip microcomputer module (602) is used for performing a function task of a lower computer of the gear switching controller (600); The second serial port module (603) is used for communication between the lower computer of the gear switching controller (600) and an upper computer; The 8-way voltage output module (604) is used for transmitting a processed gear switching parameter to the electrochemical workstation (800); The second circuit function module (605) is used for program burning, hardware reset and anti-static protection of the gear switching controller (600).

6. A fast electrochemical imaging method based on slave machine driving, the method is realized based on the system of claims 1-5, characterized in that, The method comprises the following steps: Step 1, setting experiment parameters and gear switching parameters of an interface program of the upper computer (700); Step 2, receiving the experiment parameters by the rapid imaging controller (500) and processing the experiment parameters to obtain processed experiment parameters; Step 3, receiving and transmitting the gear switching parameters by the gear switching controller (600) to control gear switching and channel start-stop of the electrochemical imaging experiment; Step 4, performing the electrochemical imaging experiment based on the processed experiment parameters and the gear switching parameters to obtain real-time position data and real-time current; Step 5, receiving and processing the real-time position data and the real-time current by the rapid imaging controller (500) and transmitting the processed data to the upper computer (700) for real-time display and storage.

7. The fast electrochemical imaging method based on lower computer driving according to claim 6, characterized in that, The experiment parameters comprise an initial voltage of a channel 1, an initial voltage of a channel 2, an infinite far distance gradual step, a feedback zone gradual step, a negative feedback stop current level, a channel 1 sensitivity, a channel 2 sensitivity, an XY imaging area, an X-axis step and a Y-axis step.

8. The fast electrochemical imaging method based on lower computer driving according to claim 6, characterized in that, The step 4 of performing the electrochemical imaging experiment based on the processed experiment parameters and the gear switching parameters comprises the following steps: Step 41, obtaining a position control signal and a voltage signal by processing the experiment parameters by the rapid imaging controller (500); Step 42, transmitting the position control signal to a piezoelectric driver (1000) based on a position control module (505), and controlling displacement of a three-dimensional piezoelectric displacement stage (901) by the piezoelectric driver (1000) using the position control signal; Step 43, the electrochemical signal control module (504) transmits the voltage signal to the electrochemical workstation (800) to apply the voltage signal to the electrochemical imaging experiment; Step 44, based on the displacement of the three-dimensional piezoelectric displacement stage (901) and the application of the voltage signal, the electrochemical imaging experiment is carried out.

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